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Reduction Kinetics of Graphene Oxide Determined by Electrical Transport Measurements and Temperature Programmed Desorption

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Reduction Kinetics of Graphene Oxide Determined by Electrical Transport Measurements and Temperature Programmed Desorption J. Phys. Chem. C XXXX, xxx, 000 A Reduction Kinetics of Graphene Oxide Determined by Electrical Transport Measurements and Temperature Programmed Desorption Inhwa Jung,† Daniel A. Field,‡ Nicholas J. Clark,‡ Yanwu Zhu,† Dongxing Yang,† Richard D. Piner,† Sasha Stankovich,§ Dmitriy A. Dikin,§ Heike Geisler,| Carl A. Ventrice, Jr.,*,‡ and Rodney S. Ruoff*,† Department of Mechanical Engineering and the Texas Materials Institute, UniVersity of Texas at Austin, Austin, Texas, 78712, Department of Physics, Texas State UniVersity, San Marcos, Texas, 78666, Department of Mechanical Engineering, Northwestern UniVersity, EVanston, Illinois, 60208, and Insitute for EnVironmental and Industrial Science, Texas State UniVersity, San Marcos, Texas, 78666 ReceiVed: May 11, 2009; ReVised Manuscript ReceiVed: August 31, 2009 The thermal stability and reduction kinetics of graphene oxide were studied by measuring the electrical resistivity of single-layer graphene films at various stages of reduction in high vacuum and by performing temperature programmed desorption (TPD) measurements of multilayer films in ultrahigh vacuum. The graphene oxide was exfoliated from the graphite oxide source material by slow-stirring in aqueous solution, which produces single-layer platelets with an average lateral size of ∼10 µm. From the TPD measurements, it was determined that the primary desorption products of the graphene oxide films for temperatures up to 300 °C are H2O, CO2, and CO, with only trace amounts of O2 being detected. Resistivity measurements on individual single-layer graphene oxide platelets resulted in an activation energy of 37 ( 1 kcal/mol. The TPD measurements of multilayer films of graphene oxide platelets give an activation energy of 32 ( 4 kcal/mol. 1. Introduction of the oxide are still debated. Some of the functional groups proposed to exist at the surfaces of graphene oxide are epoxide Graphene oxide, which is an electrical insulator, shows (C-O-C), single-bonded on-top oxygen (C-O), and hydroxyl promise for use in several technological applications. For (C-OH) groups. In addition, carbonyl (CdO) groups are instance, individual, monolayer, graphene oxide platelets could expected to form at missing carbon atom defect sites of the be used as dielectric layers in nanoscale electronic devices. Since surface, and carboxylic (OdC-OH) groups, carbonyl groups, the electrical, optical, and mechanical properties of graphene and hydroxyl groups are expected to form on the edges of the oxide can be controlled by chemical modification, films platelets. Recent solid-state NMR studies of 13C-labeled graphite composed of layers of graphene oxide platelets may be used as 23 - oxide have shed further light on this topic. the active region of chemical sensors.1 4 In principle, graphene oxide films could also be used as a precursor for the formation Before graphene oxide can be used in most technological of large-scale graphene films by either thermal or chemical applications, it is important to understand its thermal stability reduction of the graphene oxide.5-11 and reduction kinetics. For instance, the decomposition tem- Graphene oxide is formed by extensive chemical oxidation perature of graphene oxide will govern which processing Publication Date (Web): October 2, 2009 | doi: 10.1021/jp904396j of graphite to form graphite oxide12-14 followed by exfoliation techniques can be used to manufacture nanoscale electronic to monolayer thick platelets by techniques such as sonication6,15,16 devices and sensors based on this material. Despite the potential 11 technological importance of this material, there have been Downloaded by UNIV OF TEXAS AUSTIN on October 2, 2009 | http://pubs.acs.org or slow-stirring in aqueous solution. It is a nonstoichiometric relatively few studies of the thermal stability of either graphite compound; therefore, the carbon-to-oxygen (C/O) ratio depends 5,24,25 7,11,26,27 on the method of preparation and by how much the material is oxide or graphene oxide. An early study of the reduced. Previous measurements of the C/O ratio of graphene thermal decomposition of graphite oxide using gas chromatog- oxide films by X-ray photoelectron spectroscopy (XPS) have raphy found that the primary desorption products are H2O, CO2, determined that the ratio of fully oxidized graphene oxide is and CO and that the decomposition occurs over a temperature - ° 24 2:1.17 The geometric structure of fully oxidized graphene oxide range of 80 180 C. These results indicate that graphene oxide is still an open question. Several different models have been is a rather fragile material and that since there is carbon loss proposed, with some of these models predicting a planar upon reduction, the structural integrity of the carbon backbone structure,18,19 while others favor a buckled structure.17,20-22 of the graphene will most likely be compromised upon Although there is general agreement that the chemical composi- decomposition. In fact, evidence for the generation of holes in thermally expanded graphite oxide has been discussed previ- tion of graphene oxide is primarily carbon, oxygen, and 28 hydrogen, the assignment and positions of the functional groups ously. In this study, the reaction kinetics and reduction process of * To whom correspondence should be addressed. E-mail: cventrice@ graphene oxide films have been investigated using two tech- txstate.edu (C.A.V.); [email protected] (R.S.R.). niques: monitoring the resistivity of a single-layer platelet of † University of Texas at Austin. graphene oxide at various stages of reduction in high vacuum, ‡ Department of Physics, Texas State University. § Northwestern University. and temperature programmed desorption (TPD) measurements | Institute for Environmental and Industrial Science, Texas State University. of multilayer films under ultrahigh vacuum (UHV) conditions. 10.1021/jp904396j CCC: $40.75 XXXX American Chemical Society B J. Phys. Chem. C, Vol. xxx, No. xx, XXXX Jung et al. Figure 2. (a) SEM image of submonolayer coverage of slow-stirred graphene oxide platelets deposited on a Si(100) substrate and (b) optical image of a ∼9 ML thick film composed of single-layer graphene oxide platelets deposited on 300 nm SiO2/Si(100). Figure 1. Schematic of the experimental setup for (a) the resistivity measurements of an individual single-layer graphene oxide platelet and (b) the TPD measurements of multilayer graphene oxide films. A schematic of these two techniques is shown in Figure 1. For the first method, the resistivity is monitored at constant temperature as a function of time and is then repeated for different temperatures ranging from 140 to 200 °C. From the time dependence of the resistivity, the reaction order, rate Figure 3. (a) Optical image of patterned electrodes on an individual constant, and an estimated value of activation energy are graphene oxide platelet and (b) sample mounting arrangement for TPD acquired. From the TPD measurements, the relative coverage measurements of multilayer graphene oxide films. of the desorption products is determined by analyzing the areas under the partial pressure versus time curves. In addition, activation energies for decomposition of the oxide are deter- above, which contains large platelets of single-layer graphene mined with TPD by measuring the shift of the temperature at oxide, is used. This technique results in graphene oxide platelets which the maximum of the partial pressure versus temperature with an average lateral size of ∼10 µm. A scanning electron plot occurs (TM) as the heating rate () of the sample is microscope (SEM) image of a submonolayer coverage of slow- increased. From the TPD measurements, it is determined that stirred platelets on a Si(100) substrate is shown in Figure 2a. the primary desorption products of the graphene oxide films For the resistivity measurements, single-layer graphene oxide for temperatures up to 300 °C are H2O, CO2, and CO, with a films were formed by applying a droplet of the slow-stirred similar TM for all three molecular species. Activation energies graphene oxide solution on the substrate followed by dispersion of 37 ( 1 and 32 ( 4 kcal/mol are measured by resistivity of the droplet by blowing with dry N2 gas. The electrical measurements on single-layer graphene oxide and TPD mea- resistivity measurements were performed using a differential surements of multilayer films, respectively. four-point probe technique.30,31 The electrodes were formed by deposition of a Au film with a Cr buffer layer using a high- Publication Date (Web): October 2, 2009 | doi: 10.1021/jp904396j 2. Experimental Section vacuum, e-beam, evaporation system and a photolithographic technique. The Si substrates were mounted on a sample holder The graphene oxide films were deposited on SiO2/Si(100) Downloaded by UNIV OF TEXAS AUSTIN on October 2, 2009 | http://pubs.acs.org substrates from an aqueous solution of graphene oxide platelets. stage and heating of the single-layer platelets was performed The nominal thickness of the SiO overlayers was 300 nm. The inside the SEM chamber (Nova NanoSEM600, FEI Co.), which 2 × -6 graphene oxide solutions were formed by exfoliation of graphite has a base pressure of 1 10 Torr. Temperature measure- oxide, which was produced by chemical oxidation of graphite ments were performed with a thermistor that sits below the using the modified Hummers method.13 Two different methods sample (Figure 1a). To correct for the temperature differential are used by our group to exfoliate the platelets: sonication and between the front surface of the Si substrate and the bottom of slow-stirring. The exfoliation is performed on samples with a the sample holder where the thermistor is located, a calibration concentration of 1 mg of graphite oxide per 1 mL of deionized curve was measured with a thermocouple attached to the front water. The sonicated platelets are exfoliated using a 150 W of a blank substrate. Further details of the resistivity measure- 4,11 ultrasonic bath, where the signature for complete exfoliation ment procedure have been described in previous publications.
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